HRID2222041
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of {4-({4-[({4-[(E)-2-(2-ethyl-1,3-thiazol-4-yl)ethenyl]-1-phenyl-1H-pyrazol-3-yl}oxy)methyl]-2-methoxyphenoxy}methyl)-5-methyl-2-(3-nitrophenyl)-1,3-oxazole (650 mg), iron (reduced) (284 mg), calcium chloride (11 mg) and 80% ethanol (8 mL) was heated under reflux for 2 hrs. Insoluble materials were removed by celite filtration, and the filtrate was concentrated. The residue was subjected to silica gel column chromatography and eluted with ethyl acetate to give {3-[4-({4-[({4-[(E)-2-(2-ethyl-1,3-thiazol-4-yl)ethenyl]-1-phenyl-1H-pyrazol-3-yl}oxy)methyl]-2-methoxyphenoxy}methyl)-5-methyl-1,3-oxazol-2-yl]phenyl}amine as yellow amorphous form (150 mg, yield 38%).
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 2 hrs
- customInsoluble materials were removed by celite filtration
- concentrationthe filtrate was concentrated
- washeluted with ethyl acetate